US6617070B1 - Methods of detecting the onset of colloid formation in particular sulfur precipitation - Google Patents

Methods of detecting the onset of colloid formation in particular sulfur precipitation Download PDF

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Publication number
US6617070B1
US6617070B1 US09/980,313 US98031302A US6617070B1 US 6617070 B1 US6617070 B1 US 6617070B1 US 98031302 A US98031302 A US 98031302A US 6617070 B1 US6617070 B1 US 6617070B1
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chamber
onset
electrolyte
electric field
oscillating electric
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Patrick John Morrissey
Graham Edward Cooley
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Regenesys Technologies Ltd
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Regenesys Technologies Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
    • H01M10/39—Accumulators not provided for in groups H01M10/05-H01M10/34 working at high temperature
    • H01M10/3909—Sodium-sulfur cells
    • H01M10/3918—Sodium-sulfur cells characterised by the electrolyte
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
    • G01N29/02—Analysing fluids
    • G01N29/032—Analysing fluids by measuring attenuation of acoustic waves
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
    • H01M10/48—Accumulators combined with arrangements for measuring, testing or indicating the condition of cells, e.g. the level or density of the electrolyte
    • H01M10/484—Accumulators combined with arrangements for measuring, testing or indicating the condition of cells, e.g. the level or density of the electrolyte for measuring electrolyte level, electrolyte density or electrolyte conductivity
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00—Indexing codes associated with group G01N29/00
    • G01N2291/02—Indexing codes associated with the analysed material
    • G01N2291/024—Mixtures
    • G01N2291/02416—Solids in liquids
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00—Indexing codes associated with group G01N29/00
    • G01N2291/02—Indexing codes associated with the analysed material
    • G01N2291/025—Change of phase or condition
    • G01N2291/0251—Solidification, icing, curing composites, polymerisation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00—Indexing codes associated with group G01N29/00
    • G01N2291/02—Indexing codes associated with the analysed material
    • G01N2291/025—Change of phase or condition
    • G01N2291/0255—(Bio)chemical reactions, e.g. on biosensors
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00—Indexing codes associated with group G01N29/00
    • G01N2291/02—Indexing codes associated with the analysed material
    • G01N2291/025—Change of phase or condition
    • G01N2291/0256—Adsorption, desorption, surface mass change, e.g. on biosensors
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the present invention relates to a method for detecting the formation o colloidal species in solutions and in particular to a method for detecting the formation of sulfur-containing colloidal species within an aqueous solution which comprises polysulfide ions, and which may also comprise sulfide ions and/or hydroxide ions and/or sulfur.
  • U.S. Pat. No. 4,485,154 discloses an electrically rechargeable anionically active reduction-oxidation electricity storage/supply system and process using a sulfide/polysulfide anolyte reaction in one half of the cell and a halide/halogen catholyte reaction in the other half of the cell.
  • the catholyte reaction is:
  • the catholyte reaction is:
  • the sulfur in the anolyte When the system is fully charged the sulfur in the anolyte is present as sulfide ions. As the system discharges elemental sulfur is produced which then dissolves in the anolyte solution by combination with sulfide ions to form polysulfide species such as S 2 2 ⁇ , S 3 2 ⁇ , S 4 2 ⁇ and S 5 2 ⁇ . However, at a certain point in the discharge cycle there will no longer be sufficient sulfide ions present to solubilize the elemental sulfur as a polysulfide and consequently the elemental sulfur precipitates out of solution. In a solution of Na 2 S this would be expected to occur when the ratio of S/Na exceeds approximately 2.5.
  • the elemental sulphur When the ratio is equal to 2.5 the elemental sulphur is solubilized as Na 2 S 5 , however, when the ratio exceeds 2.5 the elemental sulphur can no longer be solubilized as a polysulfide and consequently precipitates but of solution. It should be, noted however that the equilibrium between sulfur and aqueous polysulfides is strongly dependent upon the alkalinity of the solution. Longer polysulfide chains may be formed in alkaline solutions thus delaying the onset of precipitation until a higher ratio of S/Na is reached.
  • charged particles such as the charged “micelle-like” structures of colloidal sulfur
  • acoustophoresis The principle of the technique is as follows. If an electric field is applied across a charged colloidal particle it will move in that field. In an oscillating electric field the motion of the particle will be proportional to the magnitude and frequency of the field. If a high frequency field is applied, and the particles respond, then high frequency motion will result. In acoustophoresis is the applied frequency is typically 10 6 Hz. Particle motion at this frequency generates a mechanical pressure wave with a magnitude characteristic of the mobility of the particle, its concentration and the density of the overall composition containing the particle.
  • ESA Electrokinetic Sonic Amplitude
  • the present invention provides a method of detecting the onset of colloid formation within a solution whose composition is in a state of change, which method comprises the steps of either
  • the method uses step (i) of the three options listed above.
  • FIG. 1 shows a schematic representation of a probe suitable for use in the present invention.
  • FIGS. 2A and 2B show the variation in ESA signal with addition of sulphur to a saturated solution of Na 2 S.
  • FIGS. 3A and 3B show the variation in ESA signal with addition of sulphur to solutions of 1.61M and 0.76M Na 2 S respectively.
  • FIG. 1 shows a schematic representation of a Matec ESA Probe.
  • the probe consists of a cylindrical tube casing ( 1 ) with two coaxial fittings at one end which allow transmission and reception from the transducer ( 2 ).
  • the transducer is a piezoelectric device mounted on one end of the probe. This is attached to one end of a delay line ( 3 ) and on the other end is a solid gold laminated electrode ( 4 ).
  • This electrode is electrically isolated from a gold cap ( 5 ) with a cross bar ( 6 ) which forms the other part of the electrode assembly.
  • the cross bar is positioned in a plane parallel to the gold electrode.
  • the gap ( ⁇ / 2 ) between the cap and the main body of the probe gives an electrode spacing of one half the acoustic wavelength in the system.
  • the acoustic delay line serves the simple purpose of separating in time the energising radiofrequency (RF) pulse from the ESA signal.
  • the head ( 7 ) of the probe is immersed in the solution to be monitored and measurements of the ESA are made. This requires two steps. Firstly, the probe needs to be calibrated, this is done by sweeping through a range of frequencies and finding the condition for the maximum in the amplitude of the received signal. The optimum frequency will vary depending on the nature of the species being detected. Secondly, after establishing the optimum frequency for the measurements the ESA measurements can be made at this frequency. Preferably the frequency is in the range of from 0.8 to 1.2 MHz. More preferably the frequency is approximately 1.0 MHz.
  • the ESA can be thought of as an apparent elastic modulus that arises from a given applied electric field. It has the dimension of Pascal per volt meter, i.e. Pa.m.V ⁇ 1 . For typical colloidal systems, the ESA obtained is in the range of mPa.m.V ⁇ 1
  • the technique commonly used involves applying an oscillating electric field to the materials and monitoring the resultant acoustic signal it will be appreciated by those skilled in the art that the technique may also be carried out either by applying an acoustic signal and monitoring the amplitude of the resultant oscillating electric field, or by applying an oscillating electric field and monitoring the amplitude of the resultant oscillating electric field.
  • the method is employed in the detection of the formation of colloids comprising sulfur within a solution comprising polysulfide ions.
  • the solution may also, comprise sulfide ions and/or hydroxide ions and/or halide ions and/or sulfur. More preferably the solution comprises one or more alkali metal cations as the counter ions to the anions listed above. Most preferably the alkali metal is sodium.
  • the method of the present invention may advantageously be employed in an electrochemical process for energy storage and/or power delivery, which process comprises the steps of:
  • FIGS. 2A and 2B Plots of the ESA signal against the mass fraction of sulphur and against the ratio of S/Na are shown in FIGS. 2A and 2B respectively.
  • a sharp increase in the slope of the FIG. 2B plot was found to occur at a ratio of S/Na of approximately 2 indicating the onset of colloid formation at this point.
  • FIGS. 3A and 3B Plots of the ESA signal against the ratio of S/Na for the 1.61M and 0.76M solutions are shown in FIGS. 3A and 3B respectively. Sharp increases in the slopes of the plots were found to occur at a ratio of S/Na of approximately 2 indicating the onset of colloid formation at this point.

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • General Chemical & Material Sciences (AREA)
  • Electrochemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Biochemistry (AREA)
  • Analytical Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Acoustics & Sound (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Colloid Chemistry (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Investigating Or Analysing Biological Materials (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
  • Glass Compositions (AREA)
  • Investigating Or Analyzing Materials By The Use Of Ultrasonic Waves (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)
  • Fuel Cell (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Hybrid Cells (AREA)
US09/980,313 1999-06-07 2000-06-07 Methods of detecting the onset of colloid formation in particular sulfur precipitation Expired - Fee Related US6617070B1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
GBGB9913185.6A GB9913185D0 (en) 1999-06-07 1999-06-07 Sulfur precipitation detector
GB9913185 1999-06-07
PCT/GB2000/002206 WO2000074839A1 (en) 1999-06-07 2000-06-07 Method of detecting the onset of colloid formation in particular suflur precipitation

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US (1) US6617070B1 (pt)
EP (1) EP1187673B1 (pt)
JP (1) JP2003501638A (pt)
KR (1) KR20020035002A (pt)
CN (1) CN1368901A (pt)
AT (1) ATE234148T1 (pt)
AU (1) AU5235800A (pt)
BG (1) BG106166A (pt)
BR (1) BR0011390A (pt)
CA (1) CA2371067A1 (pt)
CZ (1) CZ20014336A3 (pt)
DE (1) DE60001655T2 (pt)
DK (1) DK1187673T3 (pt)
ES (1) ES2194739T3 (pt)
GB (2) GB9913185D0 (pt)
HU (1) HUP0201563A2 (pt)
IL (1) IL146763A0 (pt)
NO (1) NO20015905L (pt)
NZ (1) NZ515862A (pt)
PL (1) PL351870A1 (pt)
PT (1) PT1187673E (pt)
SK (1) SK17502001A3 (pt)
WO (1) WO2000074839A1 (pt)
ZA (1) ZA200109795B (pt)

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080282778A1 (en) * 2005-10-25 2008-11-20 Freescale Semiconductor, Inc. Method For Testing a Slurry Used to Form a Semiconductor Device
US20130322903A1 (en) * 2012-05-31 2013-12-05 Christian Kopp Method to determine the mass concentration of particles in a dispersion including particles and fluid
US20200020991A1 (en) * 2017-03-31 2020-01-16 Toyota Motor Europe System and method for charge protection of a lithium-ion battery
US11608486B2 (en) 2015-07-02 2023-03-21 Terumo Bct, Inc. Cell growth with mechanical stimuli
US11613727B2 (en) 2010-10-08 2023-03-28 Terumo Bct, Inc. Configurable methods and systems of growing and harvesting cells in a hollow fiber bioreactor system
US11624046B2 (en) 2017-03-31 2023-04-11 Terumo Bct, Inc. Cell expansion
US11629332B2 (en) 2017-03-31 2023-04-18 Terumo Bct, Inc. Cell expansion
US11634677B2 (en) 2016-06-07 2023-04-25 Terumo Bct, Inc. Coating a bioreactor in a cell expansion system
US11667881B2 (en) 2014-09-26 2023-06-06 Terumo Bct, Inc. Scheduled feed
US11667876B2 (en) 2013-11-16 2023-06-06 Terumo Bct, Inc. Expanding cells in a bioreactor
US11685883B2 (en) 2016-06-07 2023-06-27 Terumo Bct, Inc. Methods and systems for coating a cell growth surface
US20230307722A1 (en) * 2016-09-09 2023-09-28 The Regents Of The University Of California Acoustic wave based dendrite prevention for rechargeable batteries
US11795432B2 (en) 2014-03-25 2023-10-24 Terumo Bct, Inc. Passive replacement of media
US11965175B2 (en) 2016-05-25 2024-04-23 Terumo Bct, Inc. Cell expansion

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU2002234424B2 (en) * 2001-02-26 2006-11-02 Agilent Technologies, Inc. Improved geometry for pulsed acoustic measurements of particle size
AUPR338101A0 (en) 2001-02-26 2001-03-22 Colloidal Dynamics Pty. Ltd. Improved geometry for pulsed acoustic measurements
DE102010041017A1 (de) * 2010-09-20 2012-03-22 Robert Bosch Gmbh Elektrische Anordnung

Citations (2)

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WO1994029694A1 (en) * 1993-06-07 1994-12-22 Colloidal Dynamics Pty. Ltd. Particle size and charge measurement in multi-component colloids
US5612148A (en) * 1994-04-13 1997-03-18 National Power Plc Process for energy storage and/or power delivery with means for restoring electrolyte balance

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US4485154A (en) * 1981-09-08 1984-11-27 Institute Of Gas Technology Electrically rechargeable anionically active reduction-oxidation electrical storage-supply system
US4497208A (en) * 1983-06-23 1985-02-05 Matec, Inc. Measurement of electro-kinetic properties of a solution
US4552019A (en) * 1984-05-21 1985-11-12 Dorr-Oliver, Incorporated Method and apparatus for measuring a colloidal potential
US5439757A (en) * 1992-10-14 1995-08-08 National Power Plc Electrochemical energy storage and/or power delivery cell with pH control
US5528133A (en) * 1994-07-21 1996-06-18 Powerpoint Technologies, Inc. Method and apparatus for determining the quality of a colloidal suspension
US5609998A (en) * 1994-12-29 1997-03-11 Eastman Kodak Company Process for dispersing concentrated aqueous slurries

Patent Citations (2)

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Publication number Priority date Publication date Assignee Title
WO1994029694A1 (en) * 1993-06-07 1994-12-22 Colloidal Dynamics Pty. Ltd. Particle size and charge measurement in multi-component colloids
US5612148A (en) * 1994-04-13 1997-03-18 National Power Plc Process for energy storage and/or power delivery with means for restoring electrolyte balance

Cited By (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080282778A1 (en) * 2005-10-25 2008-11-20 Freescale Semiconductor, Inc. Method For Testing a Slurry Used to Form a Semiconductor Device
US8061185B2 (en) * 2005-10-25 2011-11-22 Freescale Semiconductor, Inc. Method for testing a slurry used to form a semiconductor device
US11773363B2 (en) 2010-10-08 2023-10-03 Terumo Bct, Inc. Configurable methods and systems of growing and harvesting cells in a hollow fiber bioreactor system
US11613727B2 (en) 2010-10-08 2023-03-28 Terumo Bct, Inc. Configurable methods and systems of growing and harvesting cells in a hollow fiber bioreactor system
US11746319B2 (en) 2010-10-08 2023-09-05 Terumo Bct, Inc. Customizable methods and systems of growing and harvesting cells in a hollow fiber bioreactor system
US20130322903A1 (en) * 2012-05-31 2013-12-05 Christian Kopp Method to determine the mass concentration of particles in a dispersion including particles and fluid
US9097641B2 (en) * 2012-05-31 2015-08-04 OCé PRINTING SYSTEMS GMBH Method to determine the mass concentration of particles in a dispersion including particles and fluid
US11708554B2 (en) 2013-11-16 2023-07-25 Terumo Bct, Inc. Expanding cells in a bioreactor
US11667876B2 (en) 2013-11-16 2023-06-06 Terumo Bct, Inc. Expanding cells in a bioreactor
US11795432B2 (en) 2014-03-25 2023-10-24 Terumo Bct, Inc. Passive replacement of media
US11667881B2 (en) 2014-09-26 2023-06-06 Terumo Bct, Inc. Scheduled feed
US11608486B2 (en) 2015-07-02 2023-03-21 Terumo Bct, Inc. Cell growth with mechanical stimuli
US11965175B2 (en) 2016-05-25 2024-04-23 Terumo Bct, Inc. Cell expansion
US11634677B2 (en) 2016-06-07 2023-04-25 Terumo Bct, Inc. Coating a bioreactor in a cell expansion system
US11685883B2 (en) 2016-06-07 2023-06-27 Terumo Bct, Inc. Methods and systems for coating a cell growth surface
US11999929B2 (en) 2016-06-07 2024-06-04 Terumo Bct, Inc. Methods and systems for coating a cell growth surface
US20230307722A1 (en) * 2016-09-09 2023-09-28 The Regents Of The University Of California Acoustic wave based dendrite prevention for rechargeable batteries
US11702634B2 (en) 2017-03-31 2023-07-18 Terumo Bct, Inc. Expanding cells in a bioreactor
US11629332B2 (en) 2017-03-31 2023-04-18 Terumo Bct, Inc. Cell expansion
US11624046B2 (en) 2017-03-31 2023-04-11 Terumo Bct, Inc. Cell expansion
US20200020991A1 (en) * 2017-03-31 2020-01-16 Toyota Motor Europe System and method for charge protection of a lithium-ion battery

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AU5235800A (en) 2000-12-28
GB0013869D0 (en) 2000-08-02
BR0011390A (pt) 2002-03-05
DE60001655T2 (de) 2003-12-04
CA2371067A1 (en) 2000-12-14
PL351870A1 (en) 2003-06-30
CN1368901A (zh) 2002-09-11
HUP0201563A2 (en) 2002-08-28
ATE234148T1 (de) 2003-03-15
BG106166A (en) 2002-06-28
NZ515862A (en) 2003-05-30
GB2350899A (en) 2000-12-13
CZ20014336A3 (cs) 2002-05-15
GB9913185D0 (en) 1999-08-04
DE60001655D1 (de) 2003-04-17
KR20020035002A (ko) 2002-05-09
EP1187673B1 (en) 2003-03-12
ES2194739T3 (es) 2003-12-01
DK1187673T3 (da) 2003-06-30
NO20015905D0 (no) 2001-12-03
ZA200109795B (en) 2003-02-28
EP1187673A1 (en) 2002-03-20
WO2000074839A1 (en) 2000-12-14
GB2350899B (en) 2002-02-20
IL146763A0 (en) 2002-07-25
NO20015905L (no) 2002-01-24
JP2003501638A (ja) 2003-01-14
PT1187673E (pt) 2003-07-31
SK17502001A3 (sk) 2002-03-05

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